HRID1957263
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
A solution of 1.35 g of sodium ethoxide in 20 ml of anhydrous ethanol was added dropwise to 4.0 g of 3-chloro-2-(4-chloro-3-formylphenyl)-5-trifluoromethylpyridine and 2.9 g of triethyl phosphonatoacetate in 70 ml of anhydrous toluene. After stirring at about 20° C. for 44 hours, the solvent was removed. The residue was taken up in 100 ml of 10% strength hydrochloric acid and extracted three times with 100 ml of ethyl acetate each time. The combined organic phases were washed with 100 concentrated. Chromatography on silica gel with cyclohexane/ethyl acetate (10:1) resulted in 3.4 g (71%) of colorless crystals; melting point: 118°-120° C.
WORKUP
后处理
- customthe solvent was removed
- extractionextracted three times with 100 ml of ethyl acetate each time
- washThe combined organic phases were washed with 100
- concentrationconcentrated